Synthetic resin and method of making the same



125i resinous body a hyde are allowed Patented Sept. 20, 1932 ROY 1r. KIEnLnon SOs-Emmet nnw-vonxgassrenon 'ro GENERAL Emma con,- IE'ANY,A oonronnrron on new Yong:

SYNTHETIC nnsrn AND lvrn'r No Drawing. Application filed April 30,

This invention relates to new and improved moldable products or synthetic resins and the method of making the same.

In the reaction of an aromatic amine and an 5; aldehyde in acid solution the reaction must not be allowed to proceed beyond a certain point, at which point an alkali, such as caustic soda, is added to eiiect neutralization and to precipitate the condensation product which is subsequently washed to remove ex cess oi aldehyde and electrolytespresent, and

is then dried and pressed hot. The preparation of the product in this way using a strong alkali, such as caustic soda, produces a resin which does not readily lend itself to molding.

The product so prepared lacks flow andthis is' a serious draw-back whenmolding with fillers, particularly as most molding mate-- rials require fillers both from an economical V and mechanical standpoint.

I have found that the use of a milder alka line precipitating agent, such .as an alkaline earth base, when vused to precipitatethe condensation product from solution produces a having a marked improvement in the property of flow under pressure, a prodnot having much better molding properties and more uniform distribution of the resinous body among the filler particles.

In carrying out my invention 1 proceed as outlined above, but instead or using a strong alkali, such as caustic soda, 1 substitute an equivalent amount oi an alkaline earth base,

i such as lime (CaO), magnesium hydroxide, or barium hydroxide, or an equivalent amount of the respective carbonates of such alkaline earth metals suspended in water. i

As examples'of the process I cite the following: o a

Aniline, hydrochloric acid, and formaldeto interact in a' suitable con tainer in the following proportions:

1 Aniline V 1 mol {Hydrochloric acid 1 mol "Formaldehyde 1.1 mole Water 3000 ce.

The aniline and water are first mixed together then the hydrochloric acid is added and the temperature is adjusted to about 28 C. The

HOD or nume al; sins 1 929. sa a- No. 359,452'1. formaldehyde is then addedkeepingthe ternpe ratu-re. of the mixture-below l 0 C After this solution has been allowed to stand for about an hour, 1 mol ofan alkaline earth,

base, such as lime, magnesium hydroxide, or barium complete. The resulting precipitate is then freedfrom electrolytes,- lot.

v n a f u i s-a l nel i v s a y hydroxideis added. and the solution, is vigorously st rred; until neutralization is;

" r ed nd; pre sed;

r a aminea examp eeb nzi line Usingbenzidine -I employ the-following for-v inn-la; a, w

. Towi llustrate the'advantageous results-ob tained, resins formed. by the use of diti'erent'l precipitating agents, were subjected to plastrclty tests," As a plasticity test the followingwas used; The amount of 'flowofthef' resmousmaterial through a standard orifice,

under agiyen temperature and pressure, and fora given t me, was measured. f Size. o "o fi e mate y ;m 1 I l .u d' a-a-a ppro T mp ra u es? '-G- Pressure, 3,000-p u ndsrpersquare inch Time; 10 min;

Under th ese conditions the amount of flow obtained is listed beside each ofthe precipi-Q tating agentslused as shown below:

is markedly increased when a milder base,

It will be observed that the amount of flow such as the alkaline earth bases used are employed as preciptating agents, instead of a is obtained than when aproduct "strong alkali.

A point to bezn'oted is that in using an' alkaline earth base to precipitatethe con densation product a much more soluble salt, stronger base, as for instance NaOH is used. "Thisallows the'p're'; cipitate to be washed free ofthe electrolyte able under heat and alkaline earth base,

set

in aconsiderably shorter period oftime,thusi I reducing the time involved in the process which advantage, a p 7 v What I claim as new and desireto secure by Letters Patent of the United States is;

l; The process of preparing a resinous which consists in treating a primary aromatic aminewith an aldehyde in the pres-. enceof anacid' which forms an addition product'withthe amine, neutralizing the acid carrying out with an alkaline earthbase, and subjecting product the precipitate so formed to heat and pressure.

7 2. The process of preparing a resinous which consists in'treating a primary aromatic amine with. formaldehyde in the presence of an acid'which forms an addition product with the amine, neutralizing the acid with an alkaline earth base,' andsubject1ng the precipitate so formed a to i sure.

heatand pres- 3. The prooess of; resinous product/which consists in treating aniline with formaldehyde in the presenceof a min 1 eral acid, neutralizing the acid with-an alka resinous 1 tion of the condensation-productof la line earth bas ,and subjecting thepreipi t t so formed ih' a l pressure." v

The stepv inthe process o'fpreparing Y resinous productwhich consists in precipitating the moldable condensation product of a primaryaromatic amine and an aldehyde mineral acid-solution with an alkaline earth b p p v H 5. The step tating the moldable condensation product'of aniline p solution with an alkaline earth base.

6. The process of preparing a resinous productwhich consists in reacting aniline is initself. an economical V in the process of preparing a productwh ch consists in precipiand formaldehyde in mineral acid with formaldehydeinlmineral acid solution,

neutralizing the. acid with IimeQseparating the precipitate so formed, drying, and com; pressing the same under heat. 7. The product obtained by the precipitar1- mary aromatic amine and an aldehyde in a solution of acid which formsan addition product with the amine, with an alkaline earth base, which P tiS moldable under 'heat' it nd pressure. a V

8'. The product obtained" by theprecipitation ofthe condensation productof aniline 2 and formaldehyde in acid solution with an 

